Reaction conditions have been developed to coacervate 600A silica sol by urea-formaldehyde polymerization into 2 mu/m silica microspheres with a pore size of about 300A. After sintering, these particles could be packed into short 3 cm columns for use in high performance liquid chromatography (HPLC). Rapid reversed phase separations of selected mixtures of proteins and peptides using flowrates from 3-4 ml/min were performed in 2 minutes or less. Three areas of study are proposed building on these preliminary data. To permit synthesis of 1 mu/m porous microspheres, use of the Simplex optimization scheme is proposed to understand the interrelationship of reaction variables. Secondly, graft polymerization reactions with vinyl-silica and various monomers such as styrene, acrylonitrile, and vinylpyrrolidone will allow more stable packings to be developed and good chromatographic efficiency to be maintained. Thirdly, selected applications of even shorter 1 cm columns packed with these 1 mu/m particles for clinical chemistry are exemplified.